CN102030535B - Preparation method of zirconium-nitride enhanced aluminum-oxynitride composite ceramic material - Google Patents
Preparation method of zirconium-nitride enhanced aluminum-oxynitride composite ceramic material Download PDFInfo
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- CN102030535B CN102030535B CN 201010563397 CN201010563397A CN102030535B CN 102030535 B CN102030535 B CN 102030535B CN 201010563397 CN201010563397 CN 201010563397 CN 201010563397 A CN201010563397 A CN 201010563397A CN 102030535 B CN102030535 B CN 102030535B
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Abstract
The invention relates to a preparation method of zirconium-nitride enhanced aluminum-oxynitride composite ceramic material. The preparation method comprises the following steps of: (1) proportioning; (2) ultrasonically dispersing nano zirconia powder; (3) preparing the mixed slurry of aluminum oxynitride and zirconia; (4) preparing the mixed powder of aluminum oxynitride and zirconia; and (5) preparing an aluminum-nitride enhanced aluminum-oxynitride composite ceramic material. The zirconium-nitride enhanced aluminum-oxynitride ceramic material prepared by using the method has the advantage of high flexure strength.
Description
Technical field: the preparation method who the present invention relates to the high performance zirconium-nitride enhanced aluminum-oxynitride composite ceramic material of a kind of technical field of inorganic nonmetallic materials.
Background technology: γ-aluminum oxynitride spinel (Alon) is a kind of more stable aluminum oxide and the solid solution ceramic material of aluminium nitride.Because it has good optics, physics and chemistry character, has been subject to extensive concern at Material Field.The aluminium oxynitride material is not only a kind of desirable high-temperature structural ceramics and advanced refractory materials, and high-purity, fine and close aluminium oxynitride material or the preferred material of a kind of high temperature resistant infrared window and head-shield.That preparation method commonly used mainly comprises is normal pressure-sintered, hot pressed sintering and reaction sintering.Wherein, normal pressure-sintered is in sintering process, and sintered body is placed heatable kiln under normal pressure (being the natural atmosphere condition), under the heat energy effect, makes base substrate become the crystal grain combination by powder aggregates, and porous insert becomes the preparation technology of DB.Hot pressed sintering is a kind of powder or green compact than hard-to-sinter to be exerted pressure in mould, the preparation technology who heats up simultaneously.Reaction sintering is a kind of a kind of preparation technology who is accompanied by solid phase, liquid phase or gas-phase reaction in the process of sintering.No matter be normal pressure-sintered or hot pressed sintering, or reaction sintering method, the bending strength of the aluminium oxynitride stupalith that obtains is on the low side, can not satisfy the demand that modern science and technology develops rapidly.For many years, in order further to improve and improve the mechanical property of aluminium oxynitride stupalith, many research workers are by adding respectively the second-phases such as boron nitride, Sai Long, silicon carbide, to strengthen the mechanical property of aluminium oxynitride base ceramic material in the aluminium oxynitride matrix.But, DeGrain up to now.
Main purpose of the present invention is take zirconium nitride as wild phase, the higher aluminium oxynitride stupalith of preparation mechanical property.Any report that not yet prepares relevant for zirconium-nitride enhanced aluminum-oxynitride composite ceramic material at present.Thereby the present invention has promoter action to applying of aluminium oxynitride stupalith.
Summary of the invention: main purpose of the present invention provides a kind of preparation method of zirconium-nitride enhanced aluminum-oxynitride composite ceramic material, and the zirconium nitride of the method preparation strengthens the aluminium oxynitride stupalith and has the high characteristics of bending strength.
The object of the present invention is achieved like this: the preparation method of zirconium-nitride enhanced aluminum-oxynitride composite ceramic material:
1, batching: raw material is aluminium oxynitride and nano zirconium oxide powder.Wherein the mass percent of aluminium oxynitride is 80 ~ 98%, and zirconic mass percent is 20 ~ 2%, utilizes the precise electronic balance to take by weighing respectively an amount of powder according to the mentioned component proportioning, and is stand-by.An amount of ethanolic soln of weighing is stand-by again.
2, ultra-sonic dispersion nano zirconium oxide powder: the beaker of above-mentioned load weighted Zirconium powder being put into certain capacity, pour an amount of ethanolic soln into again, it is carried out supersound process, the time of ultra-sonic dispersion is 2 ~ 15 minutes, can make zirconia solution, stand-by.
3, the mixed slurry of preparation aluminium oxynitride and zirconium white formation: above-mentioned load weighted aluminium oxynitride powder is poured in the ball grinder, then in this ball grinder, pour scattered zirconia solution into, pour at last an amount of ethanolic soln into, after the glass stick stirring, put into again zirconium oxide balls, the total mass of zirconium oxide balls is 4 ~ 5:1 with the ratio of the total mass of feed oxygen aluminium nitride and zirconium white mixed powder, capping, behind the ball milling 12 ~ 48 hours, can obtain the mixed slurry that consisted of by aluminium oxynitride and zirconium white, stand-by.
4, the mixed powder of preparation aluminium oxynitride and zirconium white formation: the above-mentioned aluminium oxynitride that has obtained and zirconium white mixed slurry were processed 12 ~ 48 hours at 60 ~ 100 degrees centigrade baking oven inner drying, and the mixed powder of drying carried out milled processed, can make the mixed powder that mixes that is consisted of by aluminium oxynitride and zirconium white.
5, preparation zirconium-nitride enhanced aluminum-oxynitride composite ceramic material: the above-mentioned ground mixed powder that is made of aluminium oxynitride and zirconium white is put into graphite jig; and it is carried out the first pressing forming processes; then put it in the hot-pressed sintering furnace; with vacuum pump the air in the hot pressing furnace is extracted out first before the heating; pass into again nitrogen as shielding gas, under nitrogen atmosphere, carry out sintering and prepare zirconium-nitride enhanced aluminum-oxynitride composite ceramic material.Wherein, sintering temperature is 1700 ~ 1900 degrees centigrade, and soaking time is 20 ~ 90 minutes, and heat-up rate is 5 ~ 30 degrees centigrade of per minutes, and institute's plus-pressure is 10 ~ 40 MPas under sintering temperature.
The present invention under nitrogen atmosphere, makes zirconium white original position generation chemical reaction be transformed into zirconium nitride take aluminium oxynitride powder and Zirconium powder as raw material, and the preparation method who utilizes hot pressing and reaction sintering to combine obtains zirconium-nitride enhanced aluminum-oxynitride composite ceramic material.Because the second-phase zirconium nitride has effectively suppressed growing up of crystal grain at the even distribution of crystal boundary position and the inhibition that in sintering process crystal boundary is moved, and has played the effect of crystal grain thinning.The zirconium-nitride enhanced aluminum-oxynitride composite ceramic material of the method preparation has reduced sintering temperature effectively, has improved the bending strength of material.
Embodiment:
Embodiment 1
The preparation of zirconium-nitride enhanced aluminum-oxynitride composite ceramic material:
1, batching: weighing micron aluminium oxynitride powder 85 grams and nano zirconium oxide powder 15 grams are stand-by respectively; An amount of ethanolic soln of weighing is stand-by again.
2, ultra-sonic dispersion nano zirconium oxide powder: above-mentioned load weighted nm-class powder of zirconium oxide is put into 50 milliliters beaker, pour an amount of ethanolic soln into again, ultra-sonic dispersion 5 minutes can make zirconia solution, and is stand-by.
3, the mixed slurry of preparation aluminium oxynitride and zirconium white formation: above-mentioned load weighted aluminium oxynitride powder is poured in the ball grinder, then in this ball grinder, pour scattered nano oxidized zirconium solution into, pour at last an amount of ethanolic soln into, after the glass stick stirring, put into again the zirconium oxide balls of 500 grams, capping, ball milling 24 hours, can obtain the mixed slurry that consisted of by aluminium oxynitride and zirconium white, stand-by.
4, the mixed powder of preparation aluminium oxynitride and zirconium white formation: the above-mentioned aluminium oxynitride that has obtained and zirconium white mixed slurry were carried out drying treatment 24 hours in 80 degrees centigrade baking oven, and the mixed powder of drying carried out milled processed, can make the mixed powder that mixes that is consisted of by aluminium oxynitride and zirconium white.
5, preparation zirconium-nitride enhanced aluminum-oxynitride composite ceramic material: the above-mentioned ground mixed powder that is made of aluminium oxynitride and zirconium white is put into graphite jig; and it is carried out the first pressing forming processes; then put it in the hot-pressed sintering furnace; with vacuum pump the air in the hot pressing furnace is extracted out first before the heating; pass into again nitrogen as shielding gas; sintering temperature is 1800 degrees centigrade; soaking time is 70 minutes; heat-up rate is 10 degrees centigrade of per minutes; institute's plus-pressure is 35 MPas under sintering temperature, sample furnace cooling after sintering is finished.
Embodiment 2
The preparation of zirconium-nitride enhanced aluminum-oxynitride composite ceramic material:
1, batching: weighing micron aluminium oxynitride powder 175 grams and nano zirconium oxide powder 25 grams are stand-by respectively; An amount of ethanolic soln of weighing is stand-by again.
2, ultra-sonic dispersion nano zirconium oxide powder: above-mentioned load weighted nm-class powder of zirconium oxide is put into 100 milliliters beaker, pour an amount of ethanolic soln into again, ultra-sonic dispersion 5 minutes can make zirconia solution, and is stand-by.
3, the mixed slurry of preparation aluminium oxynitride and zirconium white formation: above-mentioned load weighted aluminium oxynitride powder is poured in the ball grinder, then in this ball grinder, pour scattered nano oxidized zirconium solution into, pour at last an amount of ethanolic soln into, after the glass stick stirring, put into again the zirconium oxide balls of 900 grams, capping, ball milling 36 hours, can obtain the mixed slurry that consisted of by aluminium oxynitride and zirconium white, stand-by.
4, the mixed powder of preparation aluminium oxynitride and zirconium white formation: the above-mentioned aluminium oxynitride that has obtained and zirconium white mixed slurry were carried out drying treatment 36 hours in 70 degrees centigrade baking oven, and the mixed powder of drying carried out milled processed, can make the mixed powder that mixes that is consisted of by aluminium oxynitride and zirconium white.
5, preparation zirconium-nitride enhanced aluminum-oxynitride composite ceramic material: the above-mentioned ground mixed powder that is made of aluminium oxynitride and zirconium white is put into graphite jig; and it is carried out the first pressing forming processes; then put it in the hot-pressed sintering furnace; with vacuum pump the air in the hot pressing furnace is extracted out first before the heating; pass into again nitrogen as shielding gas; sintering temperature is 1900 degrees centigrade; soaking time is 30 minutes; heat-up rate is 10 degrees centigrade of per minutes; institute's plus-pressure is 20 MPas under sintering temperature, sample furnace cooling after sintering is finished.
Claims (1)
1. the preparation method of a zirconium-nitride enhanced aluminum-oxynitride composite ceramic material, it is characterized in that: the preparation method is: (1), batching: raw material is aluminium oxynitride and nano zirconium oxide powder; Wherein the mass percent of aluminium oxynitride is 80 ~ 98%, and zirconic mass percent is 20 ~ 2%, utilizes the precise electronic balance to take by weighing respectively an amount of powder according to the mentioned component proportioning, and is stand-by; An amount of ethanolic soln of weighing is stand-by again; (2), ultra-sonic dispersion nano zirconium oxide powder: the beaker of above-mentioned load weighted Zirconium powder being put into certain capacity, pour an amount of ethanolic soln into again, it is carried out supersound process, the time of ultra-sonic dispersion is 2 ~ 15 minutes, can make zirconia solution, stand-by; (3), the mixed slurry of preparation aluminium oxynitride and zirconium white formation: above-mentioned load weighted aluminium oxynitride powder is poured in the ball grinder, then in this ball grinder, pour scattered zirconia solution into, pour at last an amount of ethanolic soln into, after the glass stick stirring, put into again zirconium oxide balls, the total mass of zirconium oxide balls is 4 ~ 5:1 with the ratio of the total mass of feed oxygen aluminium nitride and zirconium white mixed powder, capping, behind the ball milling 12 ~ 48 hours, can obtain the mixed slurry that consisted of by aluminium oxynitride and zirconium white, stand-by; (4), the mixed powder of preparation aluminium oxynitride and zirconium white formation: the above-mentioned aluminium oxynitride that has obtained and zirconium white mixed slurry were processed 12 ~ 48 hours at 60 ~ 100 degrees centigrade baking oven inner drying, and the mixed powder of drying carried out milled processed, can make the mixed powder that mixes that is consisted of by aluminium oxynitride and zirconium white; (5), preparation zirconium-nitride enhanced aluminum-oxynitride composite ceramic material: the above-mentioned ground mixed powder that is made of aluminium oxynitride and zirconium white is put into graphite jig, and it is carried out the first pressing forming processes, then put it in the hot-pressed sintering furnace, with vacuum pump the air in the hot pressing furnace is extracted out first before the heating, pass into again nitrogen as shielding gas, under nitrogen atmosphere, carry out sintering and prepare zirconium-nitride enhanced aluminum-oxynitride composite ceramic material; Wherein, sintering temperature is 1700 ~ 1900 degrees centigrade, and soaking time is 20 ~ 90 minutes, and heat-up rate is 5 ~ 30 degrees centigrade of per minutes, and institute's plus-pressure is 10 ~ 40 MPas under sintering temperature.
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| CN103664166B (en) * | 2013-11-28 | 2014-12-10 | 山东理工大学 | Method for preparing flaky AlON/cubic-phase ZrO2 composite material |
| CN104163631B (en) * | 2014-08-04 | 2016-04-06 | 余姚市巧迪电器厂 | A kind of zirconium nitride Quito unit nano composite ceramic mould material and preparation method thereof |
| CN110540429B (en) * | 2019-08-29 | 2022-06-14 | 南充三环电子有限公司 | Aluminum nitride sintered body and application |
| CN115650730A (en) * | 2022-05-31 | 2023-01-31 | 广东工业大学 | Aluminum nitride ceramic substrate and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5098623A (en) * | 1987-06-01 | 1992-03-24 | Svenska Keraminstitutet | Method for producing ceramic composite materials containing silicon oxynitride and zirconium oxide |
| CN1919796A (en) * | 2006-09-04 | 2007-02-28 | 青岛大学 | Oxide ceramics multiple phase refractory material |
| CN101058506A (en) * | 2007-02-12 | 2007-10-24 | 河北理工大学 | Al-AlN-ZrO2 thermal shock resistant ceramic material |
| CN101560099A (en) * | 2009-05-27 | 2009-10-21 | 东北大学 | Method for preparing ZrN-Sialon-SiC composite powder |
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| JP2000319070A (en) * | 1999-04-30 | 2000-11-21 | Nkk Corp | Impact resistant refractory and its production |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5098623A (en) * | 1987-06-01 | 1992-03-24 | Svenska Keraminstitutet | Method for producing ceramic composite materials containing silicon oxynitride and zirconium oxide |
| CN1919796A (en) * | 2006-09-04 | 2007-02-28 | 青岛大学 | Oxide ceramics multiple phase refractory material |
| CN101058506A (en) * | 2007-02-12 | 2007-10-24 | 河北理工大学 | Al-AlN-ZrO2 thermal shock resistant ceramic material |
| CN101560099A (en) * | 2009-05-27 | 2009-10-21 | 东北大学 | Method for preparing ZrN-Sialon-SiC composite powder |
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| JP特开2000-319070A 2000.11.21 |
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